中国环境监测
中國環境鑑測
중국배경감측
ENVIRONMENTAL MONITORING IN CHINA
2014年
5期
80-84
,共5页
固相萃取%超高效液相色谱-串联质谱%药物%自然水体
固相萃取%超高效液相色譜-串聯質譜%藥物%自然水體
고상췌취%초고효액상색보-천련질보%약물%자연수체
SPE%HPLC-MS-MS%pharmaceuticals%nature water
采用固相萃取-高效液相色谱-串联质谱法( SPE-UPLC-MS-MS)测定自然水体中的10种典型药物污染。比较了2种萃取柱HLB和C18的富集效果,并对水样pH、萃取柱的淋洗溶剂及水样体积进行了优化。结果表明,采用 HLB小柱进行富集净化,水样体积为500 mL,调节pH=3?0,95%甲醇洗脱,在0~200μg/L范围内10种药物的标准曲线线性关系良好( r≥0?999),方法检出限0?5~2?0 ng/L,精密度高( RSD<10%),加标回收率为64?3%~100?7%。经过对太湖和某污水厂排水口水样的测试,表明该方法适用于自然水体药物的快速检测,同时大部分药物被检出,说明选择的10种目标药物及建立的检测方法对研究中国水体药物污染具有一定的参考价值。
採用固相萃取-高效液相色譜-串聯質譜法( SPE-UPLC-MS-MS)測定自然水體中的10種典型藥物汙染。比較瞭2種萃取柱HLB和C18的富集效果,併對水樣pH、萃取柱的淋洗溶劑及水樣體積進行瞭優化。結果錶明,採用 HLB小柱進行富集淨化,水樣體積為500 mL,調節pH=3?0,95%甲醇洗脫,在0~200μg/L範圍內10種藥物的標準麯線線性關繫良好( r≥0?999),方法檢齣限0?5~2?0 ng/L,精密度高( RSD<10%),加標迴收率為64?3%~100?7%。經過對太湖和某汙水廠排水口水樣的測試,錶明該方法適用于自然水體藥物的快速檢測,同時大部分藥物被檢齣,說明選擇的10種目標藥物及建立的檢測方法對研究中國水體藥物汙染具有一定的參攷價值。
채용고상췌취-고효액상색보-천련질보법( SPE-UPLC-MS-MS)측정자연수체중적10충전형약물오염。비교료2충췌취주HLB화C18적부집효과,병대수양pH、췌취주적림세용제급수양체적진행료우화。결과표명,채용 HLB소주진행부집정화,수양체적위500 mL,조절pH=3?0,95%갑순세탈,재0~200μg/L범위내10충약물적표준곡선선성관계량호( r≥0?999),방법검출한0?5~2?0 ng/L,정밀도고( RSD<10%),가표회수솔위64?3%~100?7%。경과대태호화모오수엄배수구수양적측시,표명해방법괄용우자연수체약물적쾌속검측,동시대부분약물피검출,설명선택적10충목표약물급건립적검측방법대연구중국수체약물오염구유일정적삼고개치。
Solid-phase extraction, high performance liquid chromatography with tandem mass spectrometry were used for determination of ten typical pharmaceuticals in natural water. The extraction efficiencies of HLB and C18 cartridges were compared, and the sample pH value, elution solvent and sample volume were optimized. HLB cartridge was selected for sorption and kept the water sample volume at 500 mL. The water sample was acidified to pH 3?0, and 95% methanol was used as elution solvent. The calibration curve was linear in the range of 0-200 μg/L with correlation coefficients up to 0?999. The recovery of standard addition for the method was 64?3%-100?7% with a high precision ( RSD<10%) and a low detection limit ( LOD<2 ng/L) . The testing results of natural samples showed that the method was suitable for quick determination of pharmaceuticals in natural water body. Most select pharmaceuticals were detected, so the selected 10 compounds and its detection method could be referred in the study of pharmaceuticals pollution in natural water.